US6078135A - Method for forming a silica film on a face panel of a cathode ray tube - Google Patents
Method for forming a silica film on a face panel of a cathode ray tube Download PDFInfo
- Publication number
- US6078135A US6078135A US08/991,262 US99126297A US6078135A US 6078135 A US6078135 A US 6078135A US 99126297 A US99126297 A US 99126297A US 6078135 A US6078135 A US 6078135A
- Authority
- US
- United States
- Prior art keywords
- silica
- face panel
- colloidal solution
- tetraethyl
- film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/20—Manufacture of screens on or from which an image or pattern is formed, picked up, converted or stored; Applying coatings to the vessel
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J29/00—Details of cathode-ray tubes or of electron-beam tubes of the types covered by group H01J31/00
- H01J29/86—Vessels; Containers; Vacuum locks
- H01J29/867—Means associated with the outside of the vessel for shielding, e.g. magnetic shields
- H01J29/868—Screens covering the input or output face of the vessel, e.g. transparent anti-static coatings, X-ray absorbing layers
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1212—Zeolites, glasses
Definitions
- the present invention relates to a method for forming a silica film on a panel and, more particularly, to a method for forming a silica film, which can interrupt electron waves or prevent static electricity, on a face panel for a cathode ray tube.
- a face panel of a cathode ray tube manufactured through an assembly line goes through a coating process of a nonglare film, an antistatic film, an antireflection film, or/and an electron wave-proof film.
- U.S. Pat. No. 5,660,876 to Kojima et al. discloses a method of manufacturing a cathode ray tube with a nonglare multi-layered film comprising at least a visible light absorbing layer containing a black dye, and an antistatic layer containing an inorganic metal compound used as a conductive agent.
- U.S. Pat. No. 5,523,649 to Tong et al. discloses a video display panel having multi-layered antireflective coating.
- the U.S. Pat. No. 5,652,477 discloses a display device having a multi-layered antistatic/antireflective coating.
- the electron wave-proof film for interrupting the electron waves is usually made of a single-layered structure having a silica layer or a dual-layered structure having antistatic and silica layers.
- the antistatic layer comprises a transparent conductive coating layer made of a material selected from the group consisting of an ITO and ATO or comprises a thin metal layer made of Ag, Ag/Pd.
- the silica layer is made through a sol-gel method.
- water for a hydrolysis reaction is added to silicon alkoxide.
- Alcohol is used as common solvent of the silicon alkoxide and the water.
- acid is used as a catalyst to derive hydrolysis and polycondensation so as to form a thin film.
- the silica film is made through a sol composition, coating, drying, and heating treatment processes. That is, composition of the silica sol is realized by adding a predetermined amount of water to a precursor such as, for example, a tetraethyl-o-silicate or a tetramethyl-o-silicate so as to derive hydrolysis reaction.
- a precursor such as, for example, a tetraethyl-o-silicate or a tetramethyl-o-silicate so as to derive hydrolysis reaction.
- a common solvent such as ethanol, methanol, or butanol is further added.
- catalyst is further added to provide a sol particle structure that is suitable for being formed into thin film by a spin coating process or a dip-coating process and for accelerating hydrolysis reaction and polycondensation reaction.
- the catalyst is selected from the group consisting of organic or inorganic acids such as hydrochloric acid, nitric acid, acetic acid, and phosphoric acid, all of which have high acidity, and yet are dangerous agents that pose health risks.
- the thin film reacts to an acid-ionic group, if the thin film is a dual-layered structure, the thin film changes in physical property.
- the structure suitable for forming a thin film refers to the connecting structure of the silicate having a three-dimensional network structure or a linear structure having a siloxane bone, on one side of which a silanol group is coupled.
- the kind of alkoxide, the amount of water, and the kind of alcohol have affect on the form of the resultant sol.
- the form of the resultant sol is affected by the kind and amount of acid added as the catalyst.
- alkoxides M1 and M2 produce hydroxides through hydrolysis reactions as follows:
- Each of the hydroxides produced as in the above converts oxygen bridge into a two-component condensation product of M1-O-M2 by water condensation between the hydroxides rather than by its homo condensation, thereby being accelerated in its reaction. This can be shown as follows:
- titanium alkoxide is used as a catalyst which can accelerate polycondensation reaction of the silicate.
- Chelate derivative can be also used as the catalyst that can adjust haydrolysis reaction speed of the titanium alkoxide.
- the colloidal solution when coated on a face panel of a cathode ray tube, this becomes the silica film. That is, after the face panel is applied with the colloidal solution, it is calcinated at a temperature of about 300° C. so that the organization of the film is fined and the attachment thereof can be stabilized.
- a titanium alkoxide derivative is used to suppress deposition of a second phase of a titanium alkoxide which serves as a catalyst. Since this method does not use an acid as a catalyst, the problems of the conventional arts can be solved.
- the present invention provide a method for forming a silica film on a face panel of a cathode ray tube, comprising the steps of:
- a first composite as a starting material, having a silica-titania two component system where alcohol is added as a solvent;
- the silica-titania two-component system is selected from a group consisting of a tetraethyl-o-silicate and a tetraethyl-silicate oligomer.
- tetraethyl-silicate oligomer has a degree of polymerization of 40, 51 or 56.
- the titaniumalkoxide derivate is a titanium acetyl acetone.
- the mixture ratio of the first and second composites is in a range from 1:1 to 10:1.
- the colloidal solution is coated on a nonglare film coated on the face panel.
- a first composite was made by dispersing tetraethyl-o-silicate of 6.7 W % into the mixture.
- a second composite was made by adding acetyl acetone of 0.1 W % to titanium isopropoxide of 0.13 W %.
- the first and second composites were mixed at a 1:1 ratio. After water of 1.2 W % was added into this mixture, a colloidal solution was obtained by agitating this mixture for about 10 hours.
- the colloidal solution of 50 cc was poured onto a 10 ⁇ 10 cm 2 glass while rotating the glass at 90 rpm. While increasing the rotating speed of the glass to 150 rpm, the colloidal solution was spin-coated on the glass.
- the gel film was dried and calcinated at a temperature of 180° C. for 30 minutes, thereby obtaining a silica film.
- a first composite was made by dispersing tetraethyl-o-silicate oligomer, having a degree of polymerization of 40, of 4.8 W % into the mixture.
- a second composite was made by adding acetyl acetone of 0.09 W % to titanium isopropoxide of 0.13 W %.
- the first and second composites were mixed at a 1:1 ratio. After water of 0.9 W % was added into this mixture, a colloidal solution was obtained by agitating this mixture for about 10 hours.
- the colloidal solution of 50 cc was poured into 10 ⁇ 10 cm 2 glass while rotating the glass at 90 rpm. While increasing the rotating speed of the glass to 150 rpm, the colloidal solution was spin coated on the glass. The gel film was dried and calcinated at a temperature of 160° C. for 30 minutes, thereby obtaining a desired silica film.
- a first composite was made by dispersing tetraethyl-o-silicate oligomer, having a degree of polymerization of 51, of 3.8 W % into the mixture.
- a second composite was made by adding acetyl acetone of 0.09 W % to titanium isopropoxide 0.14 W %.
- the first and second composites were mixed at a 1:1 ratio. After water of 0.8 W % was added into this mixture, a colloidal solution was obtained by agitating this mixture for about 10 hours.
- the colloidal solution of 50 cc was poured onto a 10 ⁇ 10 cm 2 glass while rotating the glass at 90 rpm. While increasing the rotating speed of the glass to 150 rpm, the colloidal solution was spin coated on the glass. The gel film was dried and calcinated at a temperature of 160° C. for 30 minutes, thereby obtaining a desired silica film.
- a first composite was made by dispersing tetraethyl-o-silicate oligomer, having a polymerization of 56, of 3.5 W % into the mixture.
- a second composite was made by adding acetyl acetone of 0.1 W % to titanium isopropoxide of 0.14 W %.
- the first and second composites were mixed at a 1:1 ratio. After water of 0.73 W % was added into this mixture, a colloidal solution was obtained by agitating this mixture for about 10 hours.
- the colloidal solution of 50 cc was poured onto a 10 ⁇ 10 cm 2 glass while rotating the glass at 90 rpm. While increasing the rotating speed of the glass to 150 rpm, the colloidal solution was spin coated on the glass. The gel film was dried and calcinated at a temperature of 200° C. for 30 minutes, thereby obtaining a desired silica film.
- a first composite was made by dispersing tetraethyl-o-silicate oligomer, having a degree of polymerization of 56, of 4.8 W % into the mixture.
- a second composite was made by adding acetyl acetone of 0.09 W % to titanium isopropoxide of 0.13 W %.
- the first and second composites were mixed at a 10:1 ratio. After water of 0.09 W % was added into this mixture, a colloidal solution was obtained by agitating this mixture for about 10 hours.
- the colloidal solution of 50 cc was poured onto a 10 ⁇ 10 cm 2 glass while rotating the glass at 90 rpm. While increasing the rotating speed of the glass to 150 rpm, the colloidal solution was spin coated on the glass. The gel film was dried and calcinated at a temperature of 180° C. for 30 minutes, thereby obtaining a desired silica film.
- the silica films obtained through all of the above embodiments were tested.
- the silica films of the first through fifth embodiments were 10.10 ⁇ 10 3 ⁇ / ⁇ , 9.85 ⁇ 10 3 , ⁇ / ⁇ , 10.05 ⁇ 10 3 ⁇ / ⁇ , 9.9 ⁇ 10 3 ⁇ / ⁇ , 10.03 ⁇ 10 3 ⁇ / ⁇ , respectively. These values are almost similar to a value of 10 ⁇ 10 3 ⁇ / ⁇ which was obtained through a method where an acid was used as the catalyst.
- the titanium alkoxide derivate is used as the catalyst instead of acid, no health risks are posed to workers, In addition, as the temperature for calcination can be reduced, an anion base is not maintained and the interface reaction does not occur.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Silicon Compounds (AREA)
- Glass Melting And Manufacturing (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Formation Of Various Coating Films On Cathode Ray Tubes And Lamps (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Catalysts (AREA)
Abstract
Description
M1(OR)n+nH.sub.2 O→M1(OH)x(OR)n-x+xROH
M2(OR)n+nH.sub.2 O→M2(OH)x(OR)n-x +xROH
M1(OH)(OR)+M2(HO)(OR)→(OR)M1-O-M2(OR)+H.sub.2 O
Claims (8)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR1019970048098A KR100247664B1 (en) | 1997-09-22 | 1997-09-22 | Method of manufacturing a silica layer |
KR97-48098 | 1997-09-22 |
Publications (1)
Publication Number | Publication Date |
---|---|
US6078135A true US6078135A (en) | 2000-06-20 |
Family
ID=19521498
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US08/991,262 Expired - Fee Related US6078135A (en) | 1997-09-22 | 1997-12-16 | Method for forming a silica film on a face panel of a cathode ray tube |
Country Status (3)
Country | Link |
---|---|
US (1) | US6078135A (en) |
JP (1) | JPH1192145A (en) |
KR (1) | KR100247664B1 (en) |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20030195328A1 (en) * | 2002-03-20 | 2003-10-16 | Yi-Feng Wang | Catalytic systems |
US20050054862A1 (en) * | 2001-10-09 | 2005-03-10 | Cyclics Corporation | Organo-titanate catalysts for preparing pure macrocyclic oligoesters |
US20050176917A1 (en) * | 2000-09-01 | 2005-08-11 | Cyclics Corporation | Methods for converting linear polyesters to macrocyclic oligoester compositions and macrocyclic oligoesters |
US20060235185A1 (en) * | 2000-09-01 | 2006-10-19 | Cyclics Corporation | Preparation of low-acid polyalkylene terephthalate and preparation of macrocyclic polyester oligomer therefrom |
US7666517B2 (en) | 2001-06-27 | 2010-02-23 | Cyclics Corporation | Isolation, formulation, and shaping of macrocyclic oligoesters |
US7750109B2 (en) | 2000-09-01 | 2010-07-06 | Cyclics Corporation | Use of a residual oligomer recyclate in the production of macrocyclic polyester oligomer |
WO2011068271A1 (en) * | 2009-12-01 | 2011-06-09 | (주)에이씨티 | Method for manufacturing a silica powder coated with an antibacterial agent, and topical dermatological composition including same |
CN104428446A (en) * | 2012-02-28 | 2015-03-18 | 因文特兰姆知识产权管理贸易投资公司 | A zeolite coating preparation assembly and operation method |
US9561967B2 (en) | 2014-08-28 | 2017-02-07 | Inventram Fikri Mulkiyet Haklari Yonetim Ticaret Ve Yatirim Anonim Sirketi | Zeolite coating preparation assembly and operation method |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5219611A (en) * | 1991-09-30 | 1993-06-15 | Cornell Research Foundation, Inc. | Preparing densified low porosity titania sol gel forms |
US5243255A (en) * | 1990-10-24 | 1993-09-07 | Mitsubishi Denki Kabushiki Kaisha | Cathode-ray tube with low reflectivity film |
US5523649A (en) * | 1994-11-08 | 1996-06-04 | Chunghwa Picture Tubes, Ltd. | Multilayer antireflective coating for video display panel |
US5652477A (en) * | 1995-11-08 | 1997-07-29 | Chunghwa Picture Tubes, Ltd. | Multilayer antistatic/antireflective coating for display device |
US5660876A (en) * | 1991-06-07 | 1997-08-26 | Sony Corporation | Method of manufacturing cathode ray tube with a nonglare multi-layered film |
US5683952A (en) * | 1993-08-11 | 1997-11-04 | Mitsubishi Gas Chemical Company, Inc. | Titanosilicate catalyst particle |
-
1997
- 1997-09-22 KR KR1019970048098A patent/KR100247664B1/en not_active IP Right Cessation
- 1997-12-16 US US08/991,262 patent/US6078135A/en not_active Expired - Fee Related
-
1998
- 1998-02-24 JP JP10042222A patent/JPH1192145A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5243255A (en) * | 1990-10-24 | 1993-09-07 | Mitsubishi Denki Kabushiki Kaisha | Cathode-ray tube with low reflectivity film |
US5660876A (en) * | 1991-06-07 | 1997-08-26 | Sony Corporation | Method of manufacturing cathode ray tube with a nonglare multi-layered film |
US5219611A (en) * | 1991-09-30 | 1993-06-15 | Cornell Research Foundation, Inc. | Preparing densified low porosity titania sol gel forms |
US5683952A (en) * | 1993-08-11 | 1997-11-04 | Mitsubishi Gas Chemical Company, Inc. | Titanosilicate catalyst particle |
US5523649A (en) * | 1994-11-08 | 1996-06-04 | Chunghwa Picture Tubes, Ltd. | Multilayer antireflective coating for video display panel |
US5652477A (en) * | 1995-11-08 | 1997-07-29 | Chunghwa Picture Tubes, Ltd. | Multilayer antistatic/antireflective coating for display device |
Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8283437B2 (en) | 2000-09-01 | 2012-10-09 | Cyclics Corporation | Preparation of low-acid polyalkylene terephthalate and preparation of macrocyclic polyester oligomer therefrom |
US20050176917A1 (en) * | 2000-09-01 | 2005-08-11 | Cyclics Corporation | Methods for converting linear polyesters to macrocyclic oligoester compositions and macrocyclic oligoesters |
US20060235185A1 (en) * | 2000-09-01 | 2006-10-19 | Cyclics Corporation | Preparation of low-acid polyalkylene terephthalate and preparation of macrocyclic polyester oligomer therefrom |
US7750109B2 (en) | 2000-09-01 | 2010-07-06 | Cyclics Corporation | Use of a residual oligomer recyclate in the production of macrocyclic polyester oligomer |
US7767781B2 (en) | 2000-09-01 | 2010-08-03 | Cyclics Corporation | Preparation of low-acid polyalkylene terephthalate and preparation of macrocyclic polyester oligomer therefrom |
US7666517B2 (en) | 2001-06-27 | 2010-02-23 | Cyclics Corporation | Isolation, formulation, and shaping of macrocyclic oligoesters |
US20050054862A1 (en) * | 2001-10-09 | 2005-03-10 | Cyclics Corporation | Organo-titanate catalysts for preparing pure macrocyclic oligoesters |
US20050227861A1 (en) * | 2002-03-20 | 2005-10-13 | Cyclics Corporation | Catalytic systems |
US20030195328A1 (en) * | 2002-03-20 | 2003-10-16 | Yi-Feng Wang | Catalytic systems |
WO2011068271A1 (en) * | 2009-12-01 | 2011-06-09 | (주)에이씨티 | Method for manufacturing a silica powder coated with an antibacterial agent, and topical dermatological composition including same |
CN104428446A (en) * | 2012-02-28 | 2015-03-18 | 因文特兰姆知识产权管理贸易投资公司 | A zeolite coating preparation assembly and operation method |
CN104428446B (en) * | 2012-02-28 | 2016-08-24 | 因文特兰姆知识产权管理贸易投资公司 | Zeolite coating prepares assembly and operational approach |
US9561967B2 (en) | 2014-08-28 | 2017-02-07 | Inventram Fikri Mulkiyet Haklari Yonetim Ticaret Ve Yatirim Anonim Sirketi | Zeolite coating preparation assembly and operation method |
Also Published As
Publication number | Publication date |
---|---|
KR100247664B1 (en) | 2000-03-15 |
JPH1192145A (en) | 1999-04-06 |
KR19990026115A (en) | 1999-04-15 |
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